EP0231908A2 - Procédé et appareil pour réactions de saponification - Google Patents

Procédé et appareil pour réactions de saponification Download PDF

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Publication number
EP0231908A2
EP0231908A2 EP87101320A EP87101320A EP0231908A2 EP 0231908 A2 EP0231908 A2 EP 0231908A2 EP 87101320 A EP87101320 A EP 87101320A EP 87101320 A EP87101320 A EP 87101320A EP 0231908 A2 EP0231908 A2 EP 0231908A2
Authority
EP
European Patent Office
Prior art keywords
conduit
vessel
openings
acid
recirculating
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP87101320A
Other languages
German (de)
English (en)
Other versions
EP0231908A3 (fr
Inventor
Bruce A. Bereiter
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Henkel Corp
Original Assignee
Henkel Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from US06/825,390 external-priority patent/US4671892A/en
Application filed by Henkel Corp filed Critical Henkel Corp
Publication of EP0231908A2 publication Critical patent/EP0231908A2/fr
Publication of EP0231908A3 publication Critical patent/EP0231908A3/fr
Withdrawn legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D13/00—Making of soap or soap solutions in general; Apparatus therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/40—Mixing liquids with liquids; Emulsifying
    • B01F23/49—Mixing systems, i.e. flow charts or diagrams
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006—Controlling or regulating processes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T436/00—Chemistry: analytical and immunological testing
    • Y10T436/12—Condition responsive control

Definitions

  • This invention relates to a new and Improved process and apparatus for saponification reactions and the like, e.g. to produce liquid soaps, on a batch scale over a sufficiently short time Interval to effect a semicontinuous process.
  • the reaction times are In the order of about 2 - 8 minutes, and reactor vessel capacities are of about 1 - 25 gallons, or greater.
  • the chemical Industry manufactures a wide variety of liquid soaps at plant sites In large quantities for shipping in container cars, drums, etc.
  • the containers are then returned to the site and refilled. in the case of drums, they are usually washed prior to return, which creates a waste disposal problem.
  • the weight of water diluent In the liquid soap represents a transportation expense.
  • Today, the manufacture of liquid soaps used In Industry no longer poses a manufacturing problem from the chemical standpoint. The greater problem Is posed In transportation of chemically toxic wastes, and In use of reactors which are economically effective in both large and small scale manufacture of the product.
  • a process and apparatus Is provided for the batch manufacture on a seml- continuous basis for saponfication reactions and the like.
  • the reactions produce liquid products during a reaction time which varies from about 2 - 8 minutes.
  • the ingredients are added sequentially In weighed amounts to water In the reactor, and the mixture of water and Ingredients are recycled, usually continuously, to ensure adequate mixing during a predetermined reaction time set for each ingredient.
  • the recycling operation Is stopped and the liquid reactant product is fed to storage; the process is then repeated. Since the process is carried out a large number of times dally, It is preferred to employ a microprocessor to control valve on-off times to enable sequencing of reactant addition and reaction times. This reduces the possibility of operator errors and also ensures product uniformity.
  • Various techniques may be used to obtain an accurate feed of reactants and include the use of a load cell, pump rates (rpm), timed volume feed, etc. It Is to be understood, however, that the equipment can also be controlled manually, using suitable valves and pumps well known to the art.
  • the microprocessor which Is the preferred method of controlling the equipment, can be readlly selected from commercially available units by those skilled In this art. For example, using an STD bus, a main processor board, an STD bus card to control Inputs and outputs for the valves, pumps, and switches used with the equipment, and another STD bus card to read the load cell used with one embodiment of the equipment, are commercially readlly available, e.g. from Prolog, Inc., or Computer Dynamics Company.
  • the operating program which Is stored on the main processor board, can readily be prepared by one skilled In this art to operate the equipment for any process to be run In accordance with the teachings of the present Invention.
  • Typical raw materials for saponification reactions include: tall I oll, coconut oll, olelc acid, linoleic acid, saponiflable olis containing liquid oleic and linoleic acid, and cracked oils.
  • Other base chemicals include fatty acids such as butyric, caproic, caprylic, undecanoic, capric, nonanoic, lauric, myristic, palmitic, stearic, elaldlc, and mixtures thereof.
  • Alkalis suitable for the saponification reaction include NaOH, KOH, and the mono, dl, and triethanolamines.
  • Reaction temperatures usually vary from about 120°F - 140°F, however, the maximum temperature limits vary from about 70°F to about 200°F. These temperatures are achieved partly by the use of hot water and partly by the exothermic nature of the reaction.
  • the usual concentrations of ingredients are about 5:1 - 6:1 of saponifiable raw material/caustic, where the saponification number varies from about 175 - 280.
  • the amount of water used Is at least 60% of the total weight of ingredients, and typically 75% - 80% by weight of the ingredient concentration.
  • Saponifiable olis e.g., tall oil, may be employed as a 100% concentrated liquid, and the caustic is added as a 45% - 50% solution.
  • Additives such as chelates, EDTA and detergents may be used to reduce the effect of hard water Ions.
  • Solvents such as isopropyl alcohol, glycol ether and butyl acetate are useful as solvents and viscosity thinners.
  • Reactor vessel sizes of about 1 - 25 gallons are suitable for most reactions, and the only practical upper limit on reactor size Is that imposed by the economics of a large size plant. It will be appreciated that small size reactors of say 1-2 gallons are suitable for use In such diverse areas as dairies, laundries, restaurants, hotels, etc., where the raw material economics and process costs are counterbalanced by the cost of delivered liquid soap.
  • FIG. 1 One embodiment of the apparatus of this invention is shown In FIG. 1, and comprises a cone-shaped reactor vessel 10 fed from a supply tank 11 containing water 12, and from reactor tanks 13, 14 and 15.
  • a cone-shaped reactor vessel 10 fed from a supply tank 11 containing water 12, and from reactor tanks 13, 14 and 15.
  • water Prior to commencement of the reaction, water Is gravity fed and measured Into the reactor throught valve 19 and line 16, followed In sequence by the other reactants.
  • the material to be reacted, e.g. tall oil, from tank 13 Is then fed through line 17 by pump 18, to produce a measured, stoichiometric amount of reactant, and then fed through an Inlet feed pipe 20 Into the reactor vessel 10.
  • the feed pipe 20 has two sets of spaced openings 21 and 22 and a baffle plate 23 between the two sets of openings to direct the flow of water and reactants toward the sidewall of the vessel for improved circulation and mixing.
  • Each set of openings Is preferably positioned around the circumference of the conduit, more
  • a recirculating pump 30 recirculates the mixture of water and the reactant from tank 13 from the bottom of the. reactor vessel 10 and through a recirculation valve 30a to an Intermediate level of reactor vessel 10, usually Just (e.g. 2 Inches) below the liquid level of reactor vessel 10, until adequate mixing has occurred.
  • a measured quantity of caustic such as KOH Is fed from tank 14 through line 31 by pump 32, and pumped Into the reactor vessel 10.
  • Mixing by means of the recirculating pump 30 is continued.
  • a measured quantity of other components such as EDTA, chelates, detergents, solvents, thinners, etc., in tank 15 (or additional tanks, If necessary) are pumped through line 33 by pump 34 to the reactor vessel 10.
  • Mixing and reacting by means of recirculation pump 30 is continued.
  • the recirculation valve 30a is switched from the reactor vessel 10 to a storage tank 35 through line 36.
  • the liquid soap or other product which has been formed In the reactor vessel Is then pumped out of the reactor by pump 30 through line 36 and Into storage tank 35, or other containers, etc., for use.
  • the heat of reaction which has been transferred from the reactor to the storage tank can be removed for use in the building.
  • Reactor vessel 40 Is shown with conduit 41 having lower entry ports 42, 43 and 44, which lead from supply tanks 45, 46 and 47.
  • Pumps 48, 49 and 50 sequentially pump the reactants from their respective supply tanks through lines 51, 52 and 53 to the lower entry ports 42, 43 and 44.
  • Water is separately fed from a supply source (e.g., a water line) through Inlet pipe 60 and solenoid water valve 61 through entry port 62 Into pipe 41.
  • the water acts as a diluent and helps control the temperature rise of the exothermic reactions.
  • Recirculating pump 55 recirculates and mixes Ingredients from supply tanks 45, 46 and 47 through recirculating valve 56 Into reactor vessel 40 through the top thereof, as opposed to the side entry shown In FIG. 1. At the end of the reaction period, recirculating valve 56 Is shut and transfer valve 57 Is opened. This enables the liquid soap or other product which has been produced to be diverted Into storage tank 58.
  • Load cell 59 from which reactor vessel 40 and conduit 41 are suspended, controls through a microprocessor (not shown) the quantity of Ingredients added at each stage of the process by differential weight measurement.
  • FIG. 3 shows a process flow chart for the sequencing of the ingredient flow for the embodiment shown In Figure 2.
  • the numerals set forth In Figure 3 show the specific sequencing steps.
  • step 1 water flow Is commenced by microprocessor 63 which opens solenoid water valve 61 and checks the set weight through load cell 59. When the set weight equals actual weight, solenoid water valve 61 is closed.
  • step 2 ingredient 1 is fed Into the reactor by microprocessor 63 which starts feed pump 48. Again the set weight of the ingredient Is compared by microprocessor 63 with the actual reading from load cell 59. When the two weights are equal, feed pump 48 Is turned off by microprocessor 63.
  • step 4 the remaining two ingredients are added, with the same weight checking being made, as in steps 1 and 2.
  • step 4 recirculating pump 55 is started by microprocessor 63 prior to the commencement of the weighing check by microprocessor 63.. After a set period of recirculation (I.e., mixing), during which time the Ingredients have reacted, recirculating pump 55 Is stopped.
  • Step 5 Involves a transfer cycle, and here recirculating valve 56 Is closed, transfer valve 57 Is opened, and recirculating pump 55 Is started and runs until the load cell reads zero weight by comparison with the total input weight of all ingredients. Recirculating pump 55 is then stopped.
  • step 6 recirculating valve 56 Is opened and transfer valve 57 Is closed to complete an entire single operation, which as Indicated occurs during a 2 - 8 minute interval. The system then returns to step 1.
  • recirculating pump 55 could be run continuously (at low speed) when mixing Is not required to avoid frequent starts and stops and to reduce start up power requirements.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Detergent Compositions (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
EP87101320A 1986-02-03 1987-01-30 Procédé et appareil pour réactions de saponification Withdrawn EP0231908A3 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
US06/825,390 US4671892A (en) 1986-02-03 1986-02-03 Process and apparatus for saponification reactions, and the like
US07/002,822 US4789499A (en) 1986-02-03 1987-01-22 Process and apparatus for saponification reactions
US2822 1987-01-22
US825390 2001-04-03

Publications (2)

Publication Number Publication Date
EP0231908A2 true EP0231908A2 (fr) 1987-08-12
EP0231908A3 EP0231908A3 (fr) 1988-08-10

Family

ID=26670926

Family Applications (1)

Application Number Title Priority Date Filing Date
EP87101320A Withdrawn EP0231908A3 (fr) 1986-02-03 1987-01-30 Procédé et appareil pour réactions de saponification

Country Status (6)

Country Link
US (1) US4789499A (fr)
EP (1) EP0231908A3 (fr)
CN (1) CN1010031B (fr)
AU (1) AU586315B2 (fr)
BR (1) BR8700453A (fr)
IN (1) IN169180B (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3374610A4 (fr) * 2015-11-11 2019-07-31 A.P. Møller - Mærsk A/S Mélangeur et procédé de préparation d'une huile destinée à être fournie aux cylindres d'un moteur à crosse à deux temps

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5990074A (en) * 1996-03-26 1999-11-23 Colgate-Palmolive Co. Process to make soap
CN1179831C (zh) * 2000-09-22 2004-12-15 花王株式会社 一定重量制品的制造方法
CN107583559A (zh) * 2017-09-20 2018-01-16 广东丽臣奥威实业有限公司 一种高效节能的表面活性剂调整工艺
CN111111484A (zh) * 2020-01-02 2020-05-08 利穗科技(苏州)有限公司 一种协同连续pH灭活液混合系统及其应用

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1404709A (en) * 1915-06-28 1922-01-24 William B Allbright Hydrogenating apparatus
BE461608A (fr) * 1940-02-06
US2578366A (en) * 1945-02-23 1951-12-11 Procter & Gamble Continuous process for neutralizing fatty acids
US2823187A (en) * 1953-01-16 1958-02-11 Fels & Company Soap manufacture
US3522017A (en) * 1964-07-13 1970-07-28 Celanese Corp Reactor for conducting controlledtemperature gas phase reactions with mixing
US4073664A (en) * 1976-02-09 1978-02-14 Olin Corporation Automatically controlled cleaning fluid circuit for a foam generating apparatus and method
US4449828A (en) * 1980-10-27 1984-05-22 Ashland Oil, Inc. Mixing apparatus
GB2106408A (en) * 1981-08-15 1983-04-13 British Petroleum Co Plc Multi-orifice mixing device

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3374610A4 (fr) * 2015-11-11 2019-07-31 A.P. Møller - Mærsk A/S Mélangeur et procédé de préparation d'une huile destinée à être fournie aux cylindres d'un moteur à crosse à deux temps

Also Published As

Publication number Publication date
AU6821187A (en) 1987-08-06
CN1010031B (zh) 1990-10-17
IN169180B (fr) 1991-09-14
EP0231908A3 (fr) 1988-08-10
US4789499A (en) 1988-12-06
CN87101884A (zh) 1987-10-07
AU586315B2 (en) 1989-07-06
BR8700453A (pt) 1987-12-08

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